Acetone → 2,2-Dimethyl-chroman-4-one

HRID 247852

반응식

HRID 247852 반응식
O[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[CH3:11][C:12]([CH3:14])=[O:13].N1CCCC1>C1(C)C=CC=CC=1>[CH3:11][C:12]1([CH3:14])[O:13][C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:3](=[O:4])[CH2:2]1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 31268PyrrolidineHCID 68490alpha-Hydroxyacetophenone

생성물 1

HCID 74542902,2-Dimethyl-chroman-4-one수율 21.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Twenty five grams (25 g) of 2-hydroxyacetophenon, 10.7 g of acetone, and 5.5 g of pyrrolidine were added to 50 ml of toluene, and heated and refluxed. Twenty hours later, the temperature was returned to ambient temperature and the solvent was distilled off under reduced pressure, to which was added 100 ml of 1N hydrogen chloride. The extraction was carried out with 50 ml×3 of chloroform, followed by washing in water, drying over anhydrous magnesium sulfate, filtering off and condensation of the filtered solution. The residue was purified on a silica gel column the fraction containing the purified product were mixed together and the solvent therein was distilled off under reduced pressure to obtain 7 g of 3,4-dihydro-2,2-dimethyl-2H-benzo[b]pyran-4-one.

후처리

  1. temperatureheated
  2. temperaturerefluxed
  3. customTwenty hours
  4. customwas returned to ambient temperature
  5. distillationthe solvent was distilled off under reduced pressure, to which
  6. additionwas added 100 ml of 1N hydrogen chloride
  7. extractionThe extraction
  8. washby washing in water
  9. dry with materialdrying over anhydrous magnesium sulfate
  10. filtrationfiltering off
  11. customcondensation of the filtered solution
  12. customThe residue was purified on a silica gel column the fraction
  13. additioncontaining the purified product
  14. additionwere mixed together
  15. distillationthe solvent therein was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-fabe6bcff6424db1a3d54fe34d9c4a15
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05208245

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